The crystals of the title complex, cis-dichloro-(tetrakis(methylthio)-ethylene) palladium(Ⅱ) (C6H12Cl2PdS4, Mr = 389.70 ) have been synthesized and analyzed structurally by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P with a = 8.211(1), b = 8.443(1), c = 10.134(2) ? a = 78.34(1), b = 89.02(2), g = 71.06(1)? V = 649.9(2) 3, Z = 2, Dc = 1.991 g/cm3, m (MoKa) = 2.437 mm-1, F(000) = 384, R = 0.0246 and Rw = 0.0621 for 2417 observed reflections with I > 2s(I). The X-ray crystal structure analysis revealed that the palladium (Ⅱ) is coordinated to two chloride anions and one chelate ligand TMTE in a quasi-square coordination geometry. Two molecules pack in face to face forming a dimmer structure with PdPd distance 3.424 ? Detailed discussions for the structure data of the complex were given by comparing with that of the free TMTE.
Some complexs of Ag(PPh 3 ) n X( n =1,2,3;X=Cl,Br,I) were electrosynthesized using NH 4 X or I 2 in non aqueous medium, in yield >95%. The mechanism of electrochemical reaction and the effect of material ratio on the complexes have been studied. When n (PPh 3 )∶ n (NH 4 X)=3∶1, Ag(PPh 3 ) 2 X(X=Cl,Br) were obtained; when n (PPh 3 )∶ n (NH 4 I/I 2 )=1∶1, AgPPh 3 I was obtained; when n (PPh 3 )∶ n (NH 4 I)= 2∶1 or 3∶1, Ag(PPh 3 ) 3 I was obtained. This method is better than the traditional chemical synthesis.
Three thiostannates (H2en)2Sn2S6?en 1, (Hen)4Sn2S6 2 (en = ethylenediamine, a known compound) and [(H2hmda)3(Hhmda)2](Sn2S6)2 3 (hmda = hexamethylenediamine) were prepared using SnCl4?5H2O and S8 as starting materials in alkylenediamine solutions under mild solvothermal conditions. Compound 1 crystallizes in the triclinic system, space group P1 with a = 8.7491(17), b = 10.704(2), c = 12.2031(19) ?, α = 74.888(13), β = 72.998(12), γ = 89.032(15)°, V = 1052.9(3) ?3, Mr = 614.08, Z = 2, Dc = 1.937 g/cm3, μ = 2.966 mm-1, F(000) = 604, S = 1.211, R = 0.0579 and wR = 0.0770 for 3999 observed reflections with I > 2σ(I); while 3 crystallizes in the triclinic system, space group P1 with a = 9.8075(13), b = 10.8266(16), c = 14.303(2) ?, α = 88.611(10), β = 81.030(9), γ = 74.609(9)°, V = 1446.1(4) ?3, Mr = 1448.78, Z = 1, Dc = 1.664 g/cm3, μ = 2.173 mm?1, F(000) = 730, S = 1.173, R = 0.0457 and wR = 0.0667 for 5738 observed reflections with I > 2σ(I). The compounds are composed of dimeric [Sn2S6]4– anions and proto- nated alkylenediamine cations.
